CN103785310B - The preparation method of a kind of polysiloxane acid imide-PEI composite double layer hollow-fibre membrane - Google Patents
The preparation method of a kind of polysiloxane acid imide-PEI composite double layer hollow-fibre membrane Download PDFInfo
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- CN103785310B CN103785310B CN201410085395.XA CN201410085395A CN103785310B CN 103785310 B CN103785310 B CN 103785310B CN 201410085395 A CN201410085395 A CN 201410085395A CN 103785310 B CN103785310 B CN 103785310B
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Abstract
The present invention relates to UF membrane point technical field, the preparation method of particularly a kind of polysiloxane acid imide-PEI double-layer hollow fiber film.The present invention, by polyetherimde films skin coating one deck polysiloxane acid imide film, has made a kind of composite double layer hollow-fibre membrane.The Thief zone performance that the present invention is provided by the high mechanical properties that provides in conjunction with polyetherimide amine layer and high porosity and polysiloxane acid imide layer, make double-layered compound film have comparatively high-mechanical property and higher permeability energy, to meet the requirement of infiltration evaporation membrane material and performance simultaneously.
Description
Technical field
The present invention relates to UF membrane point technical field, the preparation method of particularly a kind of polysiloxane acid imide-PEI double-layer hollow fiber film.
Technical background
Along with the continuous development and progression of human civilization, the level of production and the demand to industrial products improve day by day, energy problem becomes one of bottleneck of restriction human future development.As a kind of environmentally friendly energy and material ethanol, get more and more people's extensive concerning, traditional alcohol production mode is mainly by technology such as rectifying.Many countries have started to formulate or adjustment energy policy, the research and development of bioenergy pendulum in important position.Ethanol receives much concern at present as safety, clean fuel and gasoline additive, and the fuel combination greatly developing ethanol and gasoline is imperative.Current ethanol uses mainly as gasoline additive, to reduce the discharge of soot, and can effectively reduce CO
2discharge; Ethanol has the octane number than gasoline simultaneously, and therefore ethanol can replace methyl tertiary butyl ether(MTBE) (MTBE) as the antiknock dope of gasoline.
Infiltration evaporation (PV) is as a kind of membrane separation technique of youth, because it can solve a difficult problem for the organics dehydrations such as alcohols high-efficiency environment friendly, it is considered to a kind of technological means being hopeful most to replace " rectifying ", and infiltration evaporation is also best suited for the method for large-scale production.Infiltration evaporation is the membrane separating process with phase change, it be with the steam pressure difference of different component in liquid mixture for motive force, utilize the dissolving of different component by film and the different processes realizing being separated of diffusion rate.Relative to traditional isolation technics, infiltration evaporation has the advantage of energy-saving and environmental protection, the sustainable development such as pollution-free.
Polysiloxane acid imide (PSI) is a kind of functional polymer material be synthesized into by dimethyl silicone polymer (PDMS) and aromatic polyimide (PI).PDMS is a kind of colourless, tasteless, nontoxic, not volatile thick liquid, and its production cost is low, and using method is simple.PDMS has very strong organic affinity and pliability due to it and makes it be easy to by organic infiltration, and it is a kind of hydrophobicity infiltration evaporation membrane material the most frequently used at present, and the infiltration evaporation membrane flux prepared by it is high and selective good.The silicone-containing copolymer obtained by using MOLECULE DESIGN means to select suitable monomer and crosslinking agent, can show remarkable separating effect in the separation process of organic matter/water.The infiltrating and vaporizing membrane made by PSI material be synthesized into by PDMS and PI has better separating effect relative to pure PDMS infiltration vaporization separation film.PEI (PEI) is a kind of transparent amber amorphous thermoplastic polymers material, and it has good mechanical stretch strength and modulus, creep resistant good stability of the dimension, and fire-retardant, resistance to chemical attack, can at high temperature Long-Time Service.
Two-layer compound hollow-fibre membrane obtained by coetrusion is internal layer by PEI layer, and PSI layer is outer.Wherein internal layer PSI is because it has loose porous the effect that composite membrane plays supporting layer, improves the mechanical performance of composite membrane simultaneously, can bear higher ambient pressure due to its excellent in mechanical performance.Outer PSI layer is fine and close, thin and have good separating effect and play the effect of separating layer due to it.This two-layer compound membrane structure is optimized while achieving the high separating effect of diffusion barrier and high flux effect.
Summary of the invention
The object of the present invention is to provide the preparation method of a kind of polysiloxane acid imide-PEI composite double layer hollow-fibre membrane, it effectively improves the performance of infiltration evaporation membrane material.
The object of the invention is to be realized by following approach: the preparation method of a kind of polysiloxane acid imide-PEI composite double layer hollow-fibre membrane:
A. the preparation of outer casting solution, outer casting solution is mixed by following compositions in weight percentage and forms at 40-50 DEG C: polysiloxane acid imide polymer 20-40%, additive 0-20%, solvent 60-80%; Wherein solvent is oxolane, and additive is the one in ethanol or methyl alcohol;
B. the preparation of internal layer casting solution, internal layer casting solution is mixed by following compositions in weight percentage and forms at 70-80 DEG C: polyetherimide polymer 15-20%, hydrophilic polymer 5-10%, polar solvent 75-80%; Wherein polar solvent is 1-METHYLPYRROLIDONE, and hydrophilic polymer is the one in glycerine, polyethylene glycol or polyvinylpyrrolidone;
C. the preparation of core liquid, core liquid is the mixed liquor of second alcohol and water, and wherein ethanol accounts for 20-50% by weight percentage;
D. outer casting solution, internal layer casting solution and core liquid are extruded from the exit orifice of spinning head, intermediate layer and endoporus respectively simultaneously, then it is shaping to enter outer coagulation bath phase transformation, form hollow-fibre membrane silk;
E. the film silk collected from outer coagulation bath is placed in water and soaks, then dries in atmosphere, gets product;
In described D step, the speed extruding spinning head of outer casting solution, internal layer casting solution controls respectively at 0.01-0.1ml/min and 1-2ml/min, and casting solution temperature is 30 DEG C; The flow control of core liquid is at 1-2ml/min, and core liquid temp is 25 DEG C.
As the further optimization of this programme, in described D step, film silk can by the air gap height of 2-5cm before entering coagulation bath, and before non-phase transformation, casting solution can directly contact with air.
As the further optimization of this programme, in described D step, when film silk is extruded from spinning head, can enter outer coagulation bath due to the gravity of solution self or under regulating wire winding speed to produce the impact of pulling force, its wire winding speed is 3-10m/min.
As the further optimization of this programme, in described D step, described outer coagulation bath is water, and its temperature is 25-40 DEG C.
The preparation method of a kind of polysiloxane acid imide of the present invention-PEI composite double layer hollow-fibre membrane, its method is simple to operation, is extremely applicable to suitability for industrialized production.It, by polyetherimde films skin coating one deck polysiloxane acid imide film, has made a kind of composite double layer hollow-fibre membrane, and this two-layer compound hollow-fibre membrane to can be used in infiltration evaporation process the organics dehydrations such as alcohols.
The Thief zone performance that the present invention is provided by the high mechanical properties that provides in conjunction with polyetherimide amine layer and high porosity and polysiloxane acid imide layer, make this double-layered compound film possess comparatively high-mechanical property and higher permeability energy, to meet the requirement to infiltration evaporation membrane material and performance simultaneously.
Detailed description of the invention
Embodiment one
1. the preparation of casting solution, core liquid and outer coagulation bath
Outer casting solution adopts PSI polymer, solvents tetrahydrofurane 20%, 80% mixes by weight percentage at 50 DEG C; Internal layer casting solution adopts PEI polymer, solvent N-methyl pyrilidone and additives polyvinyl alcohol three kinds of substances in percentage by weight 15%, 5%, 80% to mix at 70 DEG C; The second alcohol and water that consists of of core liquid 20%, 80% is prepared by weight percentage; Outer coagulation bath consist of water.
2. the spinning of hollow-fibre membrane
Outer casting solution is flowed out from spinning head exit orifice, and internal layer casting solution flows out from spinning head interstitial hole, and make core liquid flow out from spinning head endoporus, and inside and outside casting solution flow velocity is respectively 2ml/min and 0.01ml/min, core flow velocity is 1.5ml/min simultaneously; The film silk formed is after the air gap height of 5cm, and enter the shaping rear collection of outer coagulation bath phase transformation with the wire winding speed of freely falling body, the casting solution temperature in said process 30 DEG C, core liquid temp 25 DEG C, coagulation bath temperature is 40 DEG C.
3. hollow-fibre membrane post processing
First the film silk of collection is put into water to soak 64 hours, the polar solvent that removing is remaining, then dry in atmosphere.
Embodiment two
1. the preparation of casting solution, core liquid and outer coagulation bath
Outer casting solution adopts PSI polymer, solvents tetrahydrofurane 20%, 80% mixes by weight percentage at 50 DEG C; Internal layer casting solution adopts PEI polymer, solvent N-methyl pyrilidone and additives polyvinyl alcohol three kinds of substances in percentage by weight 15%, 5%, 80% to mix at 70 DEG C; The second alcohol and water that consists of of core liquid 20%, 80% is prepared by weight percentage; Outer coagulation bath consist of water.
2. the spinning of hollow-fibre membrane
Outer casting solution is flowed out from spinning head exit orifice, and internal layer casting solution flows out from spinning head interstitial hole, and make core liquid flow out from spinning head endoporus, and inside and outside casting solution flow velocity is respectively 2ml/min and 0.02ml/min, core flow velocity is 1.5ml/min simultaneously; The film silk formed is after the air gap height of 5cm, and enter the shaping rear collection of outer coagulation bath phase transformation with the wire winding speed of freely falling body, the casting solution temperature in said process 30 DEG C, core liquid temp 25 DEG C, coagulation bath temperature is 40 DEG C.
3. hollow-fibre membrane post processing
First the film silk of collection is put into water to soak 64 hours, the polar solvent that removing is remaining, then dry in atmosphere.
Embodiment three
1. the preparation of casting solution, core liquid and outer coagulation bath
Outer casting solution adopts PSI polymer, solvents tetrahydrofurane 20%, 80% mixes by weight percentage at 50 DEG C; Internal layer casting solution adopts PEI polymer, solvent N-methyl pyrilidone and additives polyvinyl alcohol three kinds of substances in percentage by weight 15%, 5%, 80% to mix at 70 DEG C; The second alcohol and water that consists of of core liquid 20%, 80% is prepared by weight percentage; Outer coagulation bath consist of water.
2. the spinning of hollow-fibre membrane
Outer casting solution is flowed out from spinning head exit orifice, and internal layer casting solution flows out from spinning head interstitial hole, and make core liquid flow out from spinning head endoporus, and inside and outside casting solution flow velocity is respectively 2ml/min and 0.05ml/min, core flow velocity is 1.5ml/min simultaneously; The film silk formed is after the air gap height of 5cm, and enter the shaping rear collection of outer coagulation bath phase transformation with the wire winding speed of freely falling body, the casting solution temperature in said process 30 DEG C, core liquid temp 25 DEG C, coagulation bath temperature is 40 DEG C.
3. hollow-fibre membrane post processing
First the film silk of collection is put into water to soak 64 hours, the polar solvent that removing is remaining, then dry in atmosphere.
Embodiment four
1. the preparation of casting solution, core liquid and outer coagulation bath
Outer casting solution adopts PSI polymer, solvents tetrahydrofurane 20%, 80% mixes by weight percentage at 50 DEG C; Internal layer casting solution adopts PEI polymer, solvent N-methyl pyrilidone and additives polyvinyl alcohol three kinds of substances in percentage by weight 15%, 5%, 80% to mix at 70 DEG C; The second alcohol and water that consists of of core liquid 20%, 80% is prepared by weight percentage; Outer coagulation bath consist of water.
2. the spinning of hollow-fibre membrane
Outer casting solution is flowed out from spinning head exit orifice, and internal layer casting solution flows out from spinning head interstitial hole, and make core liquid flow out from spinning head endoporus, and inside and outside casting solution flow velocity is respectively 2ml/min and 0.1ml/min, core flow velocity is 1.5ml/min simultaneously; The film silk formed is after the air gap height of 5cm, and enter the shaping rear collection of outer coagulation bath phase transformation with the wire winding speed of freely falling body, the casting solution temperature in said process 30 DEG C, core liquid temp 25 DEG C, coagulation bath temperature is 40 DEG C.
3. hollow-fibre membrane post processing
First the film silk of collection is put into water to soak 64 hours, the polar solvent that removing is remaining, then dry in atmosphere.
Embodiment five
1. the preparation of casting solution, core liquid and outer coagulation bath
Outer casting solution adopts PSI polymer, solvents tetrahydrofurane and additive ethanol 20%, 20%, 60% to mix at 50 DEG C by weight percentage; Internal layer casting solution adopts PEI polymer, solvent N-methyl pyrilidone and additives polyvinyl alcohol three kinds of substances in percentage by weight 15%, 5%, 80% to mix at 70 DEG C; The second alcohol and water that consists of of core liquid 20%, 80% is prepared by weight percentage; Outer coagulation bath consist of water.
2. the spinning of hollow-fibre membrane
Outer casting solution is flowed out from spinning head exit orifice, and internal layer casting solution flows out from spinning head interstitial hole, and make core liquid flow out from spinning head endoporus, and inside and outside casting solution flow velocity is respectively 2ml/min and 0.01ml/min, core flow velocity is 1.5ml/min simultaneously; The film silk formed is after the air gap height of 5cm, and enter the shaping rear collection of outer coagulation bath phase transformation with the wire winding speed of freely falling body, the casting solution temperature in said process 30 DEG C, core liquid temp 25 DEG C, coagulation bath temperature is 40 DEG C.
3. hollow-fibre membrane post processing
First the film silk of collection is put into water to soak 64 hours, the polar solvent that removing is remaining, then dry in atmosphere.
Embodiment six
1. the preparation of casting solution, core liquid and outer coagulation bath
Outer casting solution adopts PSI polymer, solvents tetrahydrofurane and additive ethanol 20%, 20%, 60% to mix at 50 DEG C by weight percentage; Internal layer casting solution adopts PEI polymer, solvent N-methyl pyrilidone and additives polyvinyl alcohol three kinds of substances in percentage by weight 15%, 5%, 80% to mix at 70 DEG C; The second alcohol and water that consists of of core liquid 20%, 80% is prepared by weight percentage; Outer coagulation bath consist of water.
2. the spinning of hollow-fibre membrane
Outer casting solution is flowed out from spinning head exit orifice, and internal layer casting solution flows out from spinning head interstitial hole, and make core liquid flow out from spinning head endoporus, and inside and outside casting solution flow velocity is respectively 2ml/min and 0.02ml/min, core flow velocity is 1.5ml/min simultaneously; The film silk formed is after the air gap height of 5cm, and enter the shaping rear collection of outer coagulation bath phase transformation with the wire winding speed of freely falling body, the casting solution temperature in said process 30 DEG C, core liquid temp 25 DEG C, coagulation bath temperature is 40 DEG C.
3. hollow-fibre membrane post processing
First the film silk of collection is put into water to soak 64 hours, the polar solvent that removing is remaining, then dry in atmosphere.
Embodiment seven
1. the preparation of casting solution, core liquid and outer coagulation bath
Outer casting solution adopts PSI polymer, solvents tetrahydrofurane and additive ethanol 20%, 20%, 60% to mix at 50 DEG C by weight percentage; Internal layer casting solution adopts PEI polymer, solvent N-methyl pyrilidone and additives polyvinyl alcohol three kinds of substances in percentage by weight 15%, 5%, 80% to mix at 70 DEG C; The second alcohol and water that consists of of core liquid 20%, 80% is prepared by weight percentage; Outer coagulation bath consist of water.
2. the spinning of hollow-fibre membrane
Outer casting solution is flowed out from spinning head exit orifice, and internal layer casting solution flows out from spinning head interstitial hole, and make core liquid flow out from spinning head endoporus, and inside and outside casting solution flow velocity is respectively 2ml/min and 0.05ml/min, core flow velocity is 1.5ml/min simultaneously; The film silk formed is after the air gap height of 5cm, and enter the shaping rear collection of outer coagulation bath phase transformation with the wire winding speed of freely falling body, the casting solution temperature in said process 30 DEG C, core liquid temp 25 DEG C, coagulation bath temperature is 40 DEG C.
3. hollow-fibre membrane post processing
First the film silk of collection is put into water to soak 64 hours, the polar solvent that removing is remaining, then dry in atmosphere.
Embodiment eight
1. the preparation of casting solution, core liquid and outer coagulation bath
Outer casting solution adopts PSI polymer, solvents tetrahydrofurane and additive ethanol 20%, 20%, 60% to mix at 50 DEG C by weight percentage; Internal layer casting solution adopts PEI polymer, solvent N-methyl pyrilidone and additives polyvinyl alcohol three kinds of substances in percentage by weight 15%, 5%, 80% to mix at 70 DEG C; The second alcohol and water that consists of of core liquid 20%, 80% is prepared by weight percentage; Outer coagulation bath consist of water.
2. the spinning of hollow-fibre membrane
Outer casting solution is flowed out from spinning head exit orifice, and internal layer casting solution flows out from spinning head interstitial hole, and make core liquid flow out from spinning head endoporus, and inside and outside casting solution flow velocity is respectively 2ml/min and 0.1ml/min, core flow velocity is 1.5ml/min simultaneously; The film silk formed is after the air gap height of 5cm, and enter the shaping rear collection of outer coagulation bath phase transformation with the wire winding speed of freely falling body, the casting solution temperature in said process 30 DEG C, core liquid temp 25 DEG C, coagulation bath temperature is 40 DEG C.
3. hollow-fibre membrane post processing
First the film silk of collection is put into water to soak 64 hours, the polar solvent that removing is remaining, then dry in atmosphere.
Claims (4)
1. a preparation method for polysiloxane acid imide-PEI composite double layer hollow-fibre membrane, is characterized in that:
A. the preparation of outer casting solution, outer casting solution is mixed by following compositions in weight percentage and forms at 40-50 DEG C: polysiloxane acid imide polymer 20-40%, additive 0-20%, solvent 60-80%; Wherein solvent is oxolane, and additive is the one in methyl alcohol or ethanol;
B. the preparation of internal layer casting solution, internal layer casting solution is mixed by following compositions in weight percentage and forms at 70-80 DEG C: polyetherimide polymer 15-20%, hydrophilic polymer 5-10%, polar solvent 75-80%; Wherein polar solvent is 1-METHYLPYRROLIDONE, and hydrophilic polymer is the one in glycerine, polyethylene glycol or polyvinylpyrrolidone;
C. the preparation of core liquid, core liquid is the mixed liquor of second alcohol and water, and wherein ethanol accounts for 20-50% by weight percentage;
D. outer casting solution, internal layer casting solution and core liquid are extruded from the exit orifice of spinning head, intermediate layer and endoporus respectively simultaneously, then it is shaping to enter outer coagulation bath phase transformation, form hollow-fibre membrane silk;
E. the film silk collected from outer coagulation bath is placed in water and soaks, then dries in atmosphere, gets product;
In described D step, the speed extruding spinning head of outer casting solution, internal layer casting solution controls respectively at 0.01-0.1ml/min and 1-2ml/min, and casting solution temperature is 30 DEG C; The flow control of core liquid is at 1-2ml/min, and core liquid temp is 25 DEG C.
2. the preparation method of a kind of polysiloxane acid imide as claimed in claim 1-PEI composite double layer hollow-fibre membrane, in described D step, film silk can by the air gap height of 2-10cm before entering coagulation bath, and before non-phase transformation, casting solution can directly contact with air.
3. the preparation method of a kind of polysiloxane acid imide as claimed in claim 1-PEI composite double layer hollow-fibre membrane, it is characterized in that: in described D step, when film silk is extruded from spinning head, can enter outer coagulation bath due to the gravity of solution self or under regulating wire winding speed to produce the impact of pulling force, its wire winding speed is 3-5m/min.
4. the preparation method of a kind of polysiloxane acid imide as claimed in claim 1-PEI composite double layer hollow-fibre membrane, it is characterized in that: in described D step, described outer coagulation bath is water, and its temperature is 25-40 DEG C.
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| CN105169974B (en) * | 2015-09-29 | 2017-11-14 | 清华大学 | A kind of hollow fiber nanofiltration membrane and preparation method thereof |
| CN105597555A (en) * | 2015-10-12 | 2016-05-25 | 中南大学 | Production technology of polyvinyl alcohol + polyether imide blend hollow fibrous membrane |
| CN110139888A (en) * | 2016-03-25 | 2019-08-16 | 沙特基础工业全球技术有限公司 | The composite article obtained by reactive precursor material |
| CN108714372B (en) * | 2018-05-29 | 2021-05-18 | 太原理工大学 | Treatment method for coal chemical industry wastewater |
| CN109499373B (en) * | 2018-12-04 | 2021-07-13 | 南京惟新环保装备技术研究院有限公司 | Hollow fiber pervaporation membrane and preparation method thereof |
| CN109796307B (en) * | 2019-01-29 | 2021-08-24 | 南京惟新环保装备技术研究院有限公司 | Bioethanol dehydration equipment and method based on hollow fiber pervaporation membrane |
| CN109809965B (en) * | 2019-02-28 | 2021-08-20 | 南京惟新环保装备技术研究院有限公司 | Glycerol concentration equipment and method based on hollow fiber pervaporation membrane |
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| US4900502A (en) * | 1985-08-29 | 1990-02-13 | Bend Research, Inc. | Hollow fiber annealing |
| CN101642683A (en) * | 2009-09-10 | 2010-02-10 | 杨乾 | Double-layer composite hollow fiber nano-filtration membrane and preparation method and special tool thereof |
| CN103122067A (en) * | 2013-02-05 | 2013-05-29 | 中南大学 | Polysiloxane imide segmented copolymer, asymmetric membrane and preparation methods |
| CN103406028A (en) * | 2013-07-22 | 2013-11-27 | 长沙奕景环保科技有限公司 | Polysiloxaneimide pervaporation composite membrane and preparation method thereof |
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2014
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4900502A (en) * | 1985-08-29 | 1990-02-13 | Bend Research, Inc. | Hollow fiber annealing |
| CN101642683A (en) * | 2009-09-10 | 2010-02-10 | 杨乾 | Double-layer composite hollow fiber nano-filtration membrane and preparation method and special tool thereof |
| CN103122067A (en) * | 2013-02-05 | 2013-05-29 | 中南大学 | Polysiloxane imide segmented copolymer, asymmetric membrane and preparation methods |
| CN103406028A (en) * | 2013-07-22 | 2013-11-27 | 长沙奕景环保科技有限公司 | Polysiloxaneimide pervaporation composite membrane and preparation method thereof |
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